Diphenyl sulfide → 4-Benzyloxycarbonylmethylcyclohexanone ethylene acetal

HRID 516870

반응식

HRID 516870 반응식
C1(SC2C=CC=CC=2)C=CC=CC=1.[O:14]1[C:18]2([CH2:23][CH2:22][C:21](=[CH:24][C:25]([O:27][CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[O:26])[CH2:20][CH2:19]2)[O:17][CH2:16][CH2:15]1.[H][H]>CO.[Pd].[C]>[O:14]1[C:18]2([CH2:23][CH2:22][CH:21]([CH2:24][C:25]([O:27][CH2:28][C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)=[O:26])[CH2:20][CH2:19]2)[O:17][CH2:16][CH2:15]1

참가 물질

6

반응물 3

HCID 8766Diphenyl sulfideHCID 86102242HCID 86102242, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 590090264-Benzyloxycarbonylmethylcyclohexanone ethylene acetal수율 82%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

Diphenyl sulfide (33 mg, 0.18 mmol) and 10% Pd-carbon (1.08 g) were added to a solution of benzyl 2-(1,4-dioxaspiro[4,5]decan-8-ylidene)acetate (5.0 g, 17.34 mmol) in methanol (50 ml) under a nitrogen gas stream, the atmosphere in the system was replaced five times with nitrogen gas, was then filled with hydrogen gas, followed by stirring under a hydrogen gas stream for 5 hr. The catalyst was removed by filtration through Celite pad and was washed with ethanol, and the filtrate was concentrated under reduced pressure to give the title compound as a yellow oil (4.1 g, yield 82%).

후처리

  1. customThe catalyst was removed by filtration through Celite pad
  2. washwas washed with ethanol
  3. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a4bed41fc4ca41229e4ff853442293c1
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115079B2

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